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Separation and determination method of desonide and related impurities

A desonide and impurity technology, applied in the field of analytical chemistry, can solve the problems of poor separation of degradation impurities, poor durability, harsh conditions, etc., and achieve the effects of strong specificity, good applicability and accurate results

Active Publication Date: 2020-02-18
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The USP38 version of the quality standard for desonide bulk drug uses reversed-phase high-performance liquid chromatography to detect related substances. The inventors of the application use this standard for the detection of related impurities in desonide bulk drug and its preparations. The limitations are due to: (1) The USP38 version of the quality standard for desonide raw material medicine stipulates that the particle size of the chromatographic column packing is 2.6 μm, and the pressure of the whole system is high, as high as 28MPa; (2) the USP38 version of desonide raw material drug quality standard is used According to the analysis of chromatographic conditions in the standard, the separation between the main peak of desonide and the degraded impurities of desonide is poor, and the resolution is less than 1.5; 20°C, the conditions are harsh and the durability is poor

Method used

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  • Separation and determination method of desonide and related impurities
  • Separation and determination method of desonide and related impurities
  • Separation and determination method of desonide and related impurities

Examples

Experimental program
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Effect test

Embodiment 1

[0051] The determination of embodiment 1 HPLC separation detection method of the present invention

[0052] Based on the limitations of using the USP38 version of desonide raw material drug quality standard reversed-phase liquid chromatography to determine the relevant impurities of desonide and its preparations, the inventors of the present application have repeatedly screened and finally determined the separation and determination of the reversed-phase HPLC method of the present invention. The method for neide and related impurities is specifically: prepare desonide need testing solution, adopt high-performance liquid chromatograph sample introduction analysis to measure the peak area of ​​each material in desonide need test solution, normalize or The relative content of each impurity is calculated by self-contrast method; the chromatographic column that described reverse-phase HPLC method adopts is the chromatographic column of octadecylsilane bonded silica gel filler, and t...

Embodiment 2

[0064] The detection of embodiment 2 sensitivity

[0065] Weigh an appropriate amount of desonide reference substance, ultrasonically dissolve and dilute it with 0.1% phosphoric acid aqueous solution-acetonitrile (volume ratio 60:40) to make a solution containing about 0.25 μg desonide per 1 ml, as a sensitivity test solution.

[0066] Accurately measure 10 μ l of the above-mentioned sensitivity test solution and inject it into a liquid chromatograph, measure according to the best chromatographic conditions in Example 1, and record the chromatogram, such as figure 1 shown. Depend on figure 1 It can be seen that in the sensitivity chromatogram, the desonide peak (S / N) is greater than 10.0. In the figure, the ordinate is the peak area (unit: mV / mAU), the abscissa is the time (unit: min), and the following chromatograms have no special instructions, the ordinate is the peak area (unit: mV / mAU), and the abscissa is the peak area (unit: mV / mAU). The mark is time (unit: min).

Embodiment 3

[0067] The detection of embodiment 3 desonide cream and blank matrix

[0068] Take 15g of this product, put it in a 50ml brown measuring bottle, add 15ml of 0.1% acetonitrile phosphoric acid, sonicate for 15min and shake it from time to time to completely disperse the gel, take it out and let it cool, add 5g of sodium chloride, shake well, let stand, take the supernatant The liquid was filtered, and the filtrate was used as the test solution of desonide cream. At the same time, take 15g of blank matrix, put it in a 50ml brown measuring bottle, add 15ml of 0.1% acetonitrile phosphoric acid, sonicate for 15min and shake it from time to time to completely disperse the gel, take it out and let it cool, add 5g of sodium chloride, shake well, let stand, and take the upper layer The clear liquid was filtered, and the filtrate was taken as the blank matrix test solution.

[0069] Accurately measure 10 μl each of the test solution and the blank substrate solution respectively, inject ...

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Abstract

The invention belongs to the field of analytical chemistry and in particular relates to a method for separating and determining desonide and related impurities. A separation method is characterized by adopting an acetonitrile water solution as the mobile phase to carry out elution separation based on an immobile phase, wherein the polarity of the immobile phase is smaller than that of the mobile phase. The method is used for effectively separating desonide and related impurities and is conducive to separation and purification of desonide. Reversed phase HPLC (high performance liquid chromatography) based on the separation method is characterized by adopting a high performance liquid chromatograph to analytically determine the peak area of each substance in a desonide test solution and computing the relative content of each impurity according to peak area normalization or a self-contrast method, wherein an adopted chromatographic column adopts octadecyl silane bonded silica gel fillers; the adopted mobile phase is the acetonitrile water solution. The method not only can achieve the effect of achieving effective separation of desonide and related impurities but also overcomes the defects of USP38 edition desonide API (active pharmaceutical ingredient) quality standards and is more suitable for quality control of APIs and preparations of desonide.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring desonide and related impurities. Background technique [0002] The molecular formula of desonide is C 24 h 32 o 6 , the chemical name is 11β,21-dihydroxy-16α,17-[(1-methylethylene)-dioxo]pregna-1,4-diene-3,20-dione, and its structural formula is as follows: [0003] [0004] Desonide is a glucocorticoid drug, which has anti-inflammatory, anti-allergic, anti-itching and reducing exudation effects; it can reduce and prevent tissue responses to inflammation, and can eliminate local non-infectious inflammation caused by fever, redness and Swelling, thereby reducing the manifestations of inflammation; has an immunosuppressive effect: prevents or suppresses cellular immune responses, suppresses primary immune responses. The topical preparations of desonide can be used for the treatment of various hormone-sensitive skin disease...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89
Inventor 管璐晗陈李平蒋海龙传娜赵静
Owner CHONGQING HUABANGSHENGKAI PHARM
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